CN103397356A - Non-toxic gold salt for gold plating and synthetic method thereof - Google Patents
Non-toxic gold salt for gold plating and synthetic method thereof Download PDFInfo
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Abstract
The invention discloses a non-toxic gold salt for gold plating and a synthetic method thereof. The method comprises the following steps of: (S1) adding gold chloride into 10 to 100 DEG C water while stirring; (S2) adding strong base solution into the gold chloride water solution; (S3) respectively adding a reducing agent solution and a coordination agent solution into the mixed solution, so as to obtain a clear and transparent solution, wherein the concentration of the reducing agent solution is 0.1-10mol/L, and the concentration of the coordination agent solution is 1.0-10 mol/L; and (S4) cooling the clear and transparent solution obtained in the step (S3) to 20 DEG C below zero-10 DEG C in a cooling container, adding the strong base solution into the cooled solution to separate crystal sediments out of the solution, continuously maintaining the temperature of the solution for 6-48 hours at the cooling temperature to adequately separate the crystal sediments out, and drying, thus obtaining the non-toxic gold salt for the gold plating. The non-toxic gold salt for the gold plating is nontoxic and environment-friendly and is stable in performance; and the coating of the non-toxic gold salt is has strong adhesion to different matrixes and can effectively protect the matrixes from being corroded by the external environment.
Description
Technical field
The present invention relates to the electrogilding technical field, especially relate to the golden salt of a kind of nontoxic gold-plated use and synthetic method thereof.
Background technology
China's economy grows continuously and fast always, shift to China at the center of world's production and processing industry, electroplating technology is not only played an important role in traditional industry, in new high-tech industry, as modern electronic technology, microelectronics, the more and more large effect of performance in mechanics of communication and product manufacturing.High temperature resistant, corrosion-resistant due to gold, chemical stability is good, so electrogilding has a wide range of applications in electronic industry.
The most popular electroplating technology of China is that alkaline cyanide is gold-plated at present, and the method is mainly with KAu (CN)
2As main salt, take KCN as complexing agent, free KCN can make bath stability, and anode normally dissolves, and improves cathodic polarization, and coating is careful, also need to add simultaneously some carbonate to increase the electroconductibility of plating solution in plating solution., because KCN has good complex ability and comparatively cheap, therefore extensively be subjected to the favor of most enterprises, but prussiate is highly toxic substance, and environment and human health have been caused great threat and harm.
Therefore, more and more generally adopt cyanogen-less gold liquid to carry out gold-plated, and the cyanogen-less gold liquid of existing gold-plated use is mainly sulfurous acid cyanogen-less gold liquid, thiosulfuric acid gold plating liquid and Citrate trianion cyanogen-less gold liquid.
The plating solution that Chinese patent application (application number is 02805673.6) discloses a kind of deposited Au and au-alloy with and application in preparation dentistry moulded piece.Gold exists with sulfurous acid gold complex form in plating solution.This invention except optional other metal that exists and the common additive for this class sulfurous acid gold plating solution, also contains at least a bismuth compound.This bismuth compound is coordination compound preferably, particularly contains the coordination compound of coordination forming agent NTA, HEDTA, TEPA, DTPA, EDNTA or EDTA.This bismuth additive can join plating solution in the preparation process of plating solution in, but provide a kind of plating solution of long-time running for the user, it needn't add other additive before galvanic deposit.The weak point of the method is wearing no resistance of coating, and the cost of plating solution is high.
Chinese patent application (application number is 200910066096.0) discloses a kind of citric acid gold potassium for gilding and preparation method thereof.The molecular formula of this citric acid gold potassium is KAu
2N
4C
12H
11O
8It is by gold perchloride is dissolved in the water, and repeatedly concentrated, dilution, then is prepared from Tripotassium Citrate, ethylenediamine tetraacetic acid (EDTA), propane dinitrile reaction in reactor.The weak point of the method be the raw materials propane dinitrile have certain toxicity and gold-plated after waste liquid in still contain a certain amount of CN
-
Summary of the invention
The object of the present invention is to provide the golden salt of a kind of nontoxic gold-plated use and synthetic method thereof, its stable performance, coating are strong from different matrix adhesive abilities, can effectively protect the corrosion of external environment to matrix, and environmental protection.
For achieving the above object, the present invention adopts following technical scheme:
The golden salt synthetic method of a kind of nontoxic gold-plated use, it comprises the following steps:
Step S1: under the condition that stirs, gold perchloride is added in the water of 10～100 ℃, until described gold perchloride dissolves fully;
Step S2: add strong base solution in the aqueous solution of above-mentioned gold perchloride, the pH value of regulating described mixing solutions is 7.5～14;
Step S3: be the reductant solution of 0.1mol/L～10mol/L and the coordination agent solution that concentration is 1.0mol/L～10mol/L to adding respectively concentration in described mixing solutions, fully stir, the pH value of regulator solution is 1～7, obtains the solution of clear;
Step S4: the solution of clear described in step S3 is positioned in cooling vessel and is cooled to-20～10 ℃, add strong base solution to cooled solution again, regulating the pH value is 7.5～14, make in solution and crystal settling occurs, continuation kept described solution 6～48 hours under this cooling temperature, make crystal settling fully separate out, then with described crystal settling 20～200 ℃ of oven dry, namely obtain the described nontoxic gold-plated golden salt of using.
Further, in the golden salt synthetic method of above-mentioned nontoxic gold-plated use, described strong base solution is KOH or NaOH solution.
Further, in the golden salt synthetic method of above-mentioned nontoxic gold-plated use, described reductive agent is Tripotassium Citrate or xitix, and described coordination agent is NC (CH
2)
mCOO (CH
2)
nCH
3, (m=1～20; N=0～20).
Further, in the golden salt synthetic method of above-mentioned nontoxic gold-plated use, described step S1 is specially:
Add 1.0～2.5L deionized water in reaction vessel, open and stir and heating unit, make in described reaction vessel after temperature is increased to 10～100 ℃ and add 20～60g gold perchloride, continue to keep stirring, until described gold perchloride dissolves fully.
Further, in the golden salt synthetic method of above-mentioned nontoxic gold-plated use, described step S2 is specially:
Get 12～336g highly basic, it is dissolved in 3L, the water of 40～100 ℃, be mixed with strong base solution;
Described strong base solution is slowly dropped in above-mentioned gold perchloride solution, and constantly detect the pH value of described mixing solutions in dripping described strong base solution process, until the pH value of described mixing solutions is adjusted to 7.5～14.
Further, in the golden salt synthetic method of above-mentioned nontoxic gold-plated use, described step S3 is specially:
Under agitation condition, appropriate reductive agent and coordination agent are joined in the water of 100 ℃, fully stir, make the coordination agent solution that reductant solution that concentration is 0.1mol/L～10mol/L and concentration are 1.0mol/L～10mol/L;
Described reductant solution and coordination agent solution slowly are added drop-wise in described mixing solutions, and the pH value of regulator solution is 1～7, obtains the solution of clear.
Further, in the golden salt synthetic method of above-mentioned nontoxic gold-plated use, also comprise before the oven dry of crystal settling described in described step S4:
Above-mentioned crystal settling of separating out is transferred in suction funnel, unnecessary moisture in the described crystal settling of elimination, and the solid transfer that will obtain is to container.
The present invention also provides a kind of nontoxic gold-plated golden salt of using, and its chemical formula is:
The present invention also provides a kind of nontoxic gold-plated golden salt of using, and its chemical formula is:
The present invention also provides a kind of nontoxic gold-plated golden salt of using, and its chemical formula is:
The present invention's golden salt of nontoxic gold-plated use and synthetic method asepsis environment-protecting thereof, stable performance, its coating is strong from different matrix adhesive abilities, can effectively protect the corrosion of external environment to matrix.
Description of drawings
Fig. 1 is the schematic flow sheet of the golden salt synthetic method of the nontoxic gold-plated use of the present invention.
Embodiment
, for the ease of understanding the present invention, below with reference to relevant drawings, the present invention is described more fully.Provided preferred embodiment of the present invention in accompanying drawing.But the present invention can realize in many different forms, is not limited to embodiment described herein.On the contrary, provide the purpose of these embodiment be make the understanding of disclosure of the present invention more comprehensively thorough.
See also Fig. 1, Fig. 1 is the schematic flow sheet of the golden salt synthetic method of the nontoxic gold-plated use of the present invention.The golden salt synthetic method of the nontoxic gold-plated use of the present invention comprises the following steps:
Step S1: under the condition that stirs, gold perchloride is added in the water of 10～100 ℃, until described gold perchloride dissolves fully;
Step S2: add strong base solution in the aqueous solution of above-mentioned gold perchloride, the pH value of regulating described mixing solutions is 7.5～14; In this step S2, reaction equation is:
Namely obtain containing AuO
- 2Mixing solutions.
Step S3: be the reductant solution of 0.1mol/L～10mol/L and the coordination agent solution that concentration is 1.0mol/L～10mol/L to adding respectively concentration in described mixing solutions, fully stir, the pH value of regulator solution is 1～7, obtains the solution of clear.
In this step, described reductive agent is reduced to the monovalence gold with the trivalent gold, and with coordination agent, forms title complex.
Step S4: the solution of clear described in step S3 is positioned in cooling vessel and is cooled to-20～10 ℃, add strong base solution to cooled solution again, regulating the pH value is 7.5～14, make in solution and crystal settling occurs, continuation kept described solution 6～48 hours under this cooling temperature, make crystal settling fully separate out, then with described crystal settling 20～200 ℃ of oven dry, namely obtain the described nontoxic gold-plated golden salt of using.
The chemical formula of described golden salt is
Wherein, described strong base solution is KOH or NaOH solution.
Described reductive agent is Tripotassium Citrate or xitix, and described coordination agent is NC (CH
2)
mCOO (CH
2)
nCH
3, wherein, m=1～20; N=0～20.
Described step S1 is specially:
Add 1.0～2.5L deionized water in reaction vessel, open and stir and heating unit, make in described reaction vessel after temperature is increased to 10～100 ℃ and add 20～60g gold perchloride, continue to keep stirring, until described gold perchloride dissolves fully.
Described step S2 is specially:
Get 12～336g highly basic, it is dissolved in 3L, the water of 40～100 ℃, be mixed with strong base solution;
Described strong base solution is slowly dropped in above-mentioned gold perchloride solution, and constantly detect the pH value of described mixing solutions in dripping described strong base solution process, until the pH value of described mixing solutions is adjusted to 7.5～14.
Described step S3 is specially:
Under agitation condition, appropriate reductive agent and coordination agent are joined in the water of 100 ℃, fully stir, make the coordination agent solution that reductant solution that concentration is 0.1mol/L～10mol/L and concentration are 1.0mol/L～10mol/L;
Described reductant solution and coordination agent solution slowly are added drop-wise in described mixing solutions, and the pH value of regulator solution is 1～7, obtains the solution of clear.
Also comprise before the oven dry of crystal settling described in described step S4:
Above-mentioned crystal settling of separating out is transferred in suction funnel, unnecessary moisture in the described crystal settling of elimination, and the solid transfer that will obtain is to container.
Separately, the present invention also provides a kind of nontoxic gold-plated golden salt of using, and its chemical formula is:
Wherein, m=1～20; N=0～20; Or
Monovalence gold in the golden salt of the nontoxic gold-plated use of the present invention is that the form with complex compound exists, setting up in the aqueous solution as
(wherein M is part, N
-For citrate ion or xitix radical ion) balance, so in electroplating technology, along with Au in solution
+Consumption, the existence of balance makes free Au
+Constantly supplemented, kept Au in plating solution
+Stablizing of concentration, be conducive to form the coating of densification, excellent performance.
Therefore, than prior art, the present invention has following advantages:
The raw material that the golden salt of the nontoxic gold-plated use of the present invention uses is hypotoxic; and the product that obtains is nontoxic; it is a kind of environmentally friendly product; and character is very stable; can use easily and store; use the resulting coating of the present invention's golden salt of nontoxic gold-plated use can have from different matrixes firmly adhesive ability also can reach certain bonding strength; can bear certain outer force intensity and not destroy; and dense structure, the porosity of coating are low, effectively protect the corrosion of external environment to matrix.
To sum up, the present invention's golden salt of nontoxic gold-plated use and synthetic method environmental protection thereof, stable performance, its coating is strong from different matrix adhesive abilities, can effectively protect the corrosion of external environment to matrix.
The present invention will be further described below in conjunction with specific embodiment.
Embodiment 1
Add the 1.0L deionized water in reaction vessel, open and stir and heating unit, temperature is increased to 10 ℃, add the 20g gold perchloride after temperature-stable, continue to keep stirring, until gold perchloride dissolves fully; Separately get 16.8g KOH, it is dissolved in 3L, the water of 10 ℃, be mixed with KOH solution, it is slowly dropped in above-mentioned gold perchloride solution, the limit edged is surveyed pH value, and adjusting pH value is 7.5; Separately in 3L is heated to the water of 10 ℃, add 97.32g Tripotassium Citrate and 339gNCCH under agitation condition
2COOCH
2CH
3, obtaining until completely dissolved potassium citrate solution and concentration that concentration is 0.1mol/L is the NCCH of 1.0mol/L
2COOCH
2CH
3Solution; With above-mentioned potassium citrate solution and NCCH
2COOCH
2CH
3Solution slowly is added drop-wise in above-mentioned solution, and regulating the pH value is 1, has obtained the solution of clear; The container that clear solution is housed obtained above is positioned in cooling vessel, make solution be cooled to-20 ℃, the KOH solution that adds above-mentioned preparation under the condition that stirs, regulating the pH value is 7.5, the crystal settling of white appears in solution, continuing to keep temperature is-20 ℃, keeps 6h, and crystal is separated out fully; Precipitation obtained above is transferred in suction funnel, and the moisture that elimination is unnecessary, to container, be positioned over the solid transfer that obtains in the baking oven of 20 ℃ and dry, and namely obtains final product.
Embodiment 2
Add the 1.5L deionized water in reaction vessel, open and stir and heating unit, temperature is increased to 40 ℃, add the 35g gold perchloride after temperature-stable, continue to keep stirring, until gold perchloride dissolves fully; Separately get 336g KOH, it is dissolved in 3L, the water of 40 ℃, be mixed with KOH solution, it is slowly dropped in above-mentioned gold perchloride solution, the limit edged is surveyed pH value, and adjusting pH value is 9; Separately in 3L is heated to the water of 40 ℃, add 52.84g xitix and 1395gNC (CH under agitation condition
2)
2COO (CH
2)
3CH
3, obtain until completely dissolved the NC (CH that ascorbic acid solution that concentration is 0.1mol/L and concentration are 3.0mol/L
2)
2COO (CH
2)
3CH
3Solution, with above-mentioned ascorbic acid solution and NC (CH
2)
2COO (CH
2)
3CH
3Solution slowly is added drop-wise in above-mentioned solution, and regulating the pH value is 3, has obtained the solution of clear; The container that clear solution is housed obtained above is positioned in cooling vessel, make solution be cooled to-10 ℃, the KOH solution that adds above-mentioned preparation under the condition that stirs, regulating the pH value is 10, the crystal settling of white appears in solution, continuing to keep temperature is-10 ℃, keeps 18h, and crystal is separated out fully; Precipitation obtained above is transferred in suction funnel, and the moisture that elimination is unnecessary, to container, be positioned over the solid transfer that obtains in the baking oven of 80 ℃ and dry, and namely obtains final product.
Embodiment 3
Add the 2.0L deionized water in reaction vessel, open and stir and heating unit, temperature is increased to 70 ℃, add the 45g gold perchloride after temperature-stable, continue to keep stirring, until gold perchloride dissolves fully; Separately get 12g NaOH, it is dissolved in 3L, the water of 70 ℃, be mixed with NaOH solution, it is slowly dropped in above-mentioned gold perchloride solution, the limit edged is surveyed pH value, and adjusting pH value is 12; Separately in 3L is heated to the water of 70 ℃, add 9732g Tripotassium Citrate and 2790gNC (CH under agitation condition
2)
3COO (CH
2)
2CH
3, obtain until completely dissolved the NC (CH that potassium citrate solution that concentration is 10mol/L and concentration are 6.0mol/L
2)
3COO (CH
2)
2CH
3Solution, with above-mentioned potassium citrate solution and NC (CH
2)
3COO (CH
2)
2CH
3Solution slowly is added drop-wise in above-mentioned solution, and regulating the pH value is 5, has obtained the solution of clear; The container that clear solution is housed obtained above is positioned in cooling vessel, make solution be cooled to 0 ℃, the NaOH solution that adds above-mentioned preparation under the condition that stirs, regulating the pH value is 12, the crystal settling of white appears in solution, continuing to keep temperature is 0 ℃, keeps 36h, and crystal is separated out fully; Precipitation obtained above is transferred in suction funnel, and the moisture that elimination is unnecessary, to container, be positioned over the solid transfer that obtains in the baking oven of 160 ℃ and dry, and namely obtains final product.
Embodiment 4
Add the 2.5L deionized water in reaction vessel, open and stir and heating unit, temperature is increased to 100 ℃, add the 60g gold perchloride after temperature-stable, continue to keep stirring, until gold perchloride dissolves fully; Separately get 240g NaOH, it is dissolved in 3L, the water of 100 ℃, be mixed with NaOH solution, it is slowly dropped in above-mentioned gold perchloride solution, the limit edged is surveyed pH value, and adjusting pH value is 14; Separately in 3L is heated to the water of 100 ℃, add 5284g xitix and 5910gNC (CH under agitation condition
2)
4COO (CH
2)
4CH
3, obtain until completely dissolved the NC (CH that ascorbic acid solution that concentration is 10mol/L and concentration are 10mol/L
2)
4COO (CH
2)
4CH
3Solution, with above-mentioned potassium citrate solution and NC (CH
2)
4COO (CH
2)
4CH
3Solution slowly is added drop-wise in above-mentioned solution, and regulating the pH value is 7, has obtained the solution of clear; The container that clear solution is housed obtained above is positioned in cooling vessel, make solution be cooled to 10 ℃, the NaOH solution that adds above-mentioned preparation under the condition that stirs, regulating the pH value is 14, the crystal settling of white appears in solution, continuing to keep temperature is 10 ℃, keeps 48h, and crystal is separated out fully; Precipitation obtained above is transferred in suction funnel, and the moisture that elimination is unnecessary, to container, be positioned over the solid transfer that obtains in the baking oven of 200 ℃ and dry, and namely obtains final product.
Here description of the invention and application is illustrative, not wants with scope restriction of the present invention in the above-described embodiments.Here the distortion of disclosed embodiment and change is possible, and the various parts of the replacement of embodiment and equivalence are known for those those of ordinary skill in the art.Those skilled in the art are noted that in the situation that do not break away from spirit of the present invention or essential characteristic, and the present invention can be with other form, structure, layout, ratio, and with other assembly, material and parts, realizes., in the situation that do not break away from the scope of the invention and spirit, can carry out other distortion and change to disclosed embodiment here.
Claims (10)
1. the golden salt synthetic method of nontoxic gold-plated use, is characterized in that, it comprises the following steps:
Step S1: under the condition that stirs, gold perchloride is added in the water of 10～100 ℃, until described gold perchloride dissolves fully;
Step S2: add strong base solution in the aqueous solution of above-mentioned gold perchloride, the pH value of regulating described mixing solutions is 7.5～14;
Step S3: be the reductant solution of 0.1mol/L～10mol/L and the coordination agent solution that concentration is 1.0mol/L～10mol/L to adding respectively concentration in described mixing solutions, fully stir, the pH value of regulator solution is 1～7, obtains the solution of clear;
Step S4: the solution of clear described in step S3 is positioned in cooling vessel and is cooled to-20～10 ℃, add strong base solution to cooled solution again, regulating the pH value is 7.5～14, make in solution and crystal settling occurs, continuation kept described solution 6～48 hours under this cooling temperature, make crystal settling fully separate out, then with described crystal settling 20～200 ℃ of oven dry, namely obtain the described nontoxic gold-plated golden salt of using.
2. the golden salt synthetic method of nontoxic gold-plated use according to claim 1, is characterized in that, described strong base solution is KOH or NaOH solution.
3. the golden salt synthetic method of nontoxic gold-plated use according to claim 2, is characterized in that, described reductive agent is Tripotassium Citrate or xitix, and described coordination agent is NC (CH
2)
mCOO (CH
2)
nCH
3, wherein, m=1～20; N=0～20.
4. the golden salt synthetic method of nontoxic gold-plated use according to claim 3, is characterized in that, described step S1 is specially:
Add 1.0～2.5L deionized water in reaction vessel, open and stir and heating unit, make in described reaction vessel after temperature is increased to 10～100 ℃ and add 20～60g gold perchloride, continue to keep stirring, until described gold perchloride dissolves fully.
5. the golden salt synthetic method of nontoxic gold-plated use according to claim 3, is characterized in that, described step S2 is specially:
Get 12～336g highly basic, it is dissolved in 3L, the water of 40～100 ℃, be mixed with strong base solution;
Described strong base solution is slowly dropped in above-mentioned gold perchloride solution, and constantly detect the pH value of described mixing solutions in dripping described strong base solution process, until the pH value of described mixing solutions is adjusted to 7.5～14.
6. the golden salt synthetic method of nontoxic gold-plated use according to claim 3, is characterized in that, described step S3 is specially:
Under agitation condition, appropriate reductive agent and coordination agent are joined in the water of 100 ℃, fully stir, make the coordination agent solution that reductant solution that concentration is 0.1mol/L～10mol/L and concentration are 1.0mol/L～10mol/L;
Described reductant solution and coordination agent solution slowly are added drop-wise in described mixing solutions, and the pH value of regulator solution is 1～7, obtains the solution of clear.
7. the golden salt synthetic method of nontoxic gold-plated use according to claim 3, is characterized in that, also comprises before the oven dry of crystal settling described in described step S4:
Above-mentioned crystal settling of separating out is transferred in suction funnel, unnecessary moisture in the described crystal settling of elimination, and the solid transfer that will obtain is to container.
8. the nontoxic gold-plated golden salt of using, is characterized in that, its chemical formula is:
9. the nontoxic gold-plated golden salt of using, is characterized in that, its chemical formula is:
10. the nontoxic gold-plated golden salt of using, is characterized in that, its chemical formula is:
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